CN102218123A - Quality control method for liver soothing and qi regulating pill - Google Patents

Abstract

The invention relates to a quality control method for a liver soothing and qi regulating pill. The method comprises the following steps: first, identifying a sample microscopic form through a microscopic identification; then identifying whether a refining prescription contains components of tree peony bark and corydalis tuber, etc. through a thin layer chromatography. According to the invention, based on an original standard of the liver soothing and qi regulating pill, microscopic characteristic descriptions of a portion of the medicinal ingredients (bunge cherry seed, magnolia officinalis, grass-leaved sweetflag rhizome, cardamom and kaladana) are revised; a thin layer chromatography of tree peony bark and corydalis tuber is established; methods with good reappearance, strong specialization, intelligible spot coloration and easily determined result are screened and included into the standard. The revised quality standard enhances medicine quality control, so that qualitative determination and quantitative determination of medicine are more accurate, and medicine quality is easier to control.

Description

The method of quality control of pill for soothing liver and regulating qi

Technical field

The invention belongs to technical field of Chinese medicines, relate to the detection method of Chinese medicine, especially the method for quality control of pill for soothing liver and regulating qi.

Background technology

The main component and the content of pill for soothing liver and regulating qi are as follows:

Rhizoma Cyperi (processed with vinegar) 96g Cortex Magnoliae Officinalis(processed with ginger) 96g Fructus Aurantii Immaturus (parched with bran) 96g Radix Gentianae 64g

Stir-baked PERICARPIUM CITRI RETICULATAE VIRIDE with vinegar 64g Fructus Amomi Rotundus 48g Radix Aucklandiae 48g Pericarpium Citri Reticulatae 32g

Vinegar Rhizoma Corydalis 32g Radix Curcumae 32g Rhizoma Acori Graminei 32g Oletum Trogopterori (vinegar system) 32g

Stir-baked RHIIZOMA CURCUMAE with vinegar 32g Cortex Moutan 32g Semen Pharbitidis (parched) 32g Radix Paeoniae Alba 32g

Rhizoma Curcumae Longae 24g Flos Magnoliae Officinalis 18g Semen Pruni 16g Lignum Aquilariae Resinatum 16g

Semen Raphani (parched) 8g

More than 20 simply, be ground into fine powder, sieve, mixing is used water pill, two layers of outermosts are with sucrose solution (1: 2) coating, drying, polishing, promptly.

Function with cure mainly: the dissipating depression of QI of having a respite, invigorating the stomach and promoting digestion is used for two side of body distensions, unhappy in the heart, vomiting is felt sick, QI rising in reverse order has some setbacks, fall full noisy, dyspepsia, constipation due to dry stool.

Pharmacological action: pharmacological research confirms, Rhizoma Cyperi, Fructus Aurantii Immaturus, Cortex Magnoliae Officinalis, Pericarpium Citri Reticulatae, Pericarpium Citri Reticulatae Viride, the Radix Aucklandiae etc. among the we, gastrointestinal smooth muscle had dual regulation, compatibility can be corrected gastrointestinal dysfunction mutually, and wherein Cortex Magnoliae Officinalis, Pericarpium Citri Reticulatae etc. all have the obvious suppression effect to the zoopery peptic ulcer.Rhizoma Corydalis, Radix Curcumae, Cortex Moutan, Oletum Trogopterori etc. can improve organizes microcirculation, helps damaging the reparation of gastric mucosa, and Pericarpium Citri Reticulatae, Pericarpium Citri Reticulatae Viride, the Radix Paeoniae Alba, Radix Gentianae etc. can increase biliary secretion, alleviate the infringement of four carbonoxides to liver.Semen Raphani, Fructus Amomi Rotundus etc. can secrete by facilitating digestion liquid, increase the gastrointestinal digestive function.So all medicines share, have hepatoprotective and protect stomach, the analgesic effect helps digestion.

According to the retrieval, not about any patent documentation of pill for soothing liver and regulating qi, there is not patent documentation certainly at present about the pill for soothing liver and regulating qi detection method yet.

Summary of the invention

The object of the present invention is to provide a kind of method of quality control of pill for soothing liver and regulating qi that can the qualitative detection ingredient, this method has that detection means is simple, testing result characteristic of accurate more.

The objective of the invention is to be achieved through the following technical solutions:

A kind of method of quality control of pill for soothing liver and regulating qi, the step of its method is:

(1) microscopical identification;

(2) with the paeonol be reference substance, adopt thin layer chromatography to differentiate in the pill for soothing liver and regulating qi prescription whether contain Cortex Moutan;

(3) with the Rhizoma Corydalis be control medicinal material, adopt thin layer chromatography to differentiate in the pill for soothing liver and regulating qi prescription whether contain Rhizoma Corydalis.

And the method for described microscopical identification is:

Get the pill for soothing liver and regulating qi sample, put microscopically and observe: plant the faint yellow or yellowish-brown of skin stone cell, shell-like, wall is thicker, and pit is obvious on one side for broad; Stone cell divides dendritic, wall thickness, and laminated striation is obvious; Fibre bundle is faint yellow, and peripheral cell contains prism of calcium oxalate, forms crystalline cellulose; Endotesta prothenchyma (of wood) yellowish-brown or brownish red, the class polygon is seen on the surface, and wall thickness, cell contain siliceous; Plant skin palisade cells light brown or brown, long 48～80 μ m.

And described thin layer chromatography differentiates that the method for Cortex Moutan in the prescription is:

1. the preparation of need testing solution: get the pill for soothing liver and regulating qi sample, porphyrize adds diethyl ether, and supersound process filters, and filtering residue is standby, and filtrate volatilizes, and residue adds acetic acid ethyl dissolution, as need testing solution;

2. the preparation of reference substance solution: get the paeonol reference substance, add acetone and make the solution that every 1ml contains 2mg, in contrast product solution;

3. thin layer condition: draw above-mentioned test sample and negative sample solution each 2～4 μ l, reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: ethyl acetate=3: 1 is developing solvent, launch, take out, dry, spray is with the tart 5% ferric chloride alcoholic solution of hydrochloric acid, inspect in the test sample chromatograph with the corresponding position of reference substance chromatograph on whether show the speckle of same color, determine whether contain the Cortex Moutan composition in the test agent;

And described thin layer chromatography differentiates that the method for Rhizoma Corydalis in the prescription is:

1. the preparation of need testing solution: get the pill for soothing liver and regulating qi sample, porphyrize adds diethyl ether, and supersound process filters, and gets filtering residue, volatilizes solvent, adds methanol 50ml, and supersound process 30 minutes filters, and filtrate evaporate to dryness, residue add methanol makes dissolving, as need testing solution;

2. the preparation of control medicinal material solution: get Rhizoma Corydalis control medicinal material 1g, add methanol 10ml, make control medicinal material solution with this step method 1.;

3. thin layer condition and result: draw each 2～6 μ l of above-mentioned three kinds of solution, put on same silica gel g thin-layer plate respectively, with n-butyl alcohol: glacial acetic acid: water=7: 1: 2 is developing solvent, launch, take out, dry, put inspect under the ultra-violet lamp 365nm in the test sample chromatograph with the corresponding position of control medicinal material chromatograph on whether show the fluorescence speckle of same color, determine whether contain the Rhizoma Corydalis composition in the test agent.

Advantage of the present invention and good effect are:

The present invention is directed to pill for soothing liver and regulating qi on the primary standard basis, having revised the microscopic features of part flavour of a drug (Semen Pruni, Cortex Magnoliae Officinalis, Rhizoma Acori Graminei, Fructus Amomi Rotundus, Semen Pharbitidiss) describes, Rhizoma Corydalis, Cortex Moutan thin layer discrimination method have been set up, filter out that favorable reproducibility, specificity are strong, the speckle colour developing is clear, method that the result easily judges is included revised quality standard in the standard in, improved the quality control of medicine, make the qualitative and detection by quantitative of medicine more accurate, quality is more prone to control.

Description of drawings

Fig. 1 is the kind skin stone cell of Semen Pruni in the micro measurement of the present invention;

Fig. 2 is the stone cell of Cortex Magnoliae Officinalis in the micro measurement of the present invention;

The crystalline cellulose of Rhizoma Acori Graminei in Fig. 3 micro measurement of the present invention;

Fig. 4 is the crystalline cellulose of Rhizoma Acori Graminei in the micro measurement of the present invention;

Fig. 5 is the endotesta prothenchyma (of wood) of Fructus Amomi Rotundus in the micro measurement of the present invention;

Fig. 6 is the kind skin palisade cells of Semen Pharbitidis in the micro measurement of the present invention;

Fig. 7 is the thin-layer chromatogram of the Yantai plate in the Cortex Moutan discriminating of the present invention, wherein from left to right: negative sample, A098033, A098044, A098045, C098070, D098080, D098083, A098085, paeonol reference substance (middle inspection institute) (T=18.7 ℃, RH=36%);

Fig. 8 is the thin-layer chromatogram of the Yantai plate in the Rhizoma Corydalis discriminating, wherein, from left to right: negative sample, Rhizoma Corydalis control medicinal material (middle inspection institute) A098033, A098044, A098045, C098070, D098080, D098083, A098085 (T=17.7 ℃, RH=38%).

The specific embodiment

Below in conjunction with embodiment, the present invention is further described, and following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.

The situation explanation that the sample that present embodiment adopts is, sample collection is detailed as table 1:

Table 1 sample collection detail

A kind of method of quality control of pill for soothing liver and regulating qi, the step of its method is:

One, microscopical identification:

(1) microscopical identification: get the pill for soothing liver and regulating qi sample, put microscopically and observe: plant the faint yellow or yellowish-brown of skin stone cell, shell-like, wall is thicker, and broad is pit obvious (Semen Pruni) on one side; Stone cell divides dendritic, wall thickness, and laminated striation is (Cortex Magnoliae Officinalis) obviously; Fibre bundle is faint yellow, and peripheral cell contains prism of calcium oxalate, forms crystalline cellulose (Rhizoma Acori Graminei); Endotesta prothenchyma (of wood) yellowish-brown or brownish red, the class polygon is seen on the surface, and wall thickness, cell contain siliceous (Fructus Amomi Rotundus); Plant skin palisade cells light brown or brown, long 48～80 μ m (Semen Pharbitidis).7 batch samples all have the microscopic features of pill for soothing liver and regulating qi in the table 1, and are up to specification, the results are shown in Figure 1 to Fig. 6.

Two, thin layer is differentiated

(1) Cortex Moutan: adopting thin layer chromatography, is reference substance with the paeonol, differentiates Cortex Moutan in the prescription.

1. the preparation of need testing solution: get pill for soothing liver and regulating qi sample 10g, porphyrize, the 50ml that adds diethyl ether, supersound process 10 minutes filters, filtering residue standby (discriminating is used as water soluble ingredient), filtrate volatilizes, and residue adds ethyl acetate 2ml makes dissolving, as need testing solution.

2. the preparation of reference substance solution: get the paeonol reference substance, add acetone and make the solution that every 1ml contains 2mg, in contrast product solution;

3. the preparation of negative sample solution: by the prescription proportioning, get other medical materials except that Cortex Moutan, make preparation by former medicine preparation technology, according to this step 1. the method extraction down of test sample item prepare, as negative sample solution;

4. thin layer condition: according to thin layer chromatography (appendix VI B) test, draw above-mentioned test sample and negative sample solution each 2～4 μ l, reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: ethyl acetate=3: 1 is developing solvent, launch, take out, dry, spray is with the tart 5% ferric chloride alcoholic solution of hydrochloric acid.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color, negative sample is noiseless, seven batch samples are all up to specification, the results are shown in Figure 7;

(2) Rhizoma Corydalis: adopting thin layer chromatography, is control medicinal material with the Rhizoma Corydalis, differentiates Rhizoma Corydalis in the prescription.

1. the preparation of need testing solution: get the filtering residue (contain Rhizoma Corydalis and be about 0.4g) under the Cortex Moutan discriminating item, volatilize solvent, add methanol 50ml, supersound process 30 minutes filters, and filtrate evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution;

2. the preparation of control medicinal material solution: get Rhizoma Corydalis control medicinal material 1g, add methanol 10ml, make control medicinal material solution with this step method 1.;

3. the preparation of negative sample solution: by the prescription proportioning, get other medical materials except that Rhizoma Corydalis, make preparation, according to the method preparation of getting under the Radix Aucklandiae, Cortex Magnoliae Officinalis and Flos Magnoliae Officinalis, the Rhizoma Cyperi item, as negative sample solution by former medicine preparation technology;

4. thin layer condition and result: according to thin layer chromatography (appendix VI B) test, draw each 2～6 μ l of above-mentioned three kinds of solution, put on same silica gel g thin-layer plate respectively, with n-butyl alcohol: glacial acetic acid: water=7: 1: 2 is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color, negative sample is noiseless, seven batch samples are all up to specification, the results are shown in Figure 8.

Wherein, all carried out serviceability test in the detection of (2) Cortex Moutan and (3) Rhizoma Corydalis, the result shows, no matter is that the result that two kinds of lamellae kinds, source or humidity detect this method influences less or not influence.

Claims (4)

1. the method for quality control of a pill for soothing liver and regulating qi, it is characterized in that: the step of its method is:

(1) microscopical identification;

(2) with the paeonol be reference substance, adopt thin layer chromatography to differentiate in the pill for soothing liver and regulating qi prescription whether contain Cortex Moutan;

(3) with the Rhizoma Corydalis be control medicinal material, adopt thin layer chromatography to differentiate in the pill for soothing liver and regulating qi prescription whether contain Rhizoma Corydalis.

2. the method for quality control of a kind of pill for soothing liver and regulating qi according to claim 1, it is characterized in that: the method for described microscopical identification is:

Get the pill for soothing liver and regulating qi sample, put microscopically and observe: plant the faint yellow or yellowish-brown of skin stone cell, shell-like, wall is thicker, and pit is obvious on one side for broad; Stone cell divides dendritic, wall thickness, and laminated striation is obvious; Fibre bundle is faint yellow, and peripheral cell contains prism of calcium oxalate, forms crystalline cellulose; Endotesta prothenchyma (of wood) yellowish-brown or brownish red, the class polygon is seen on the surface, and wall thickness, cell contain siliceous; Plant skin palisade cells light brown or brown, long 48～80 μ m.

3. the method for quality control of a kind of pill for soothing liver and regulating qi according to claim 1 is characterized in that: described thin layer chromatography differentiates that the method for Cortex Moutan in the prescription is:

1. the preparation of need testing solution: get the pill for soothing liver and regulating qi sample, porphyrize adds diethyl ether, and supersound process filters, and filtering residue is standby, and filtrate volatilizes, and residue adds acetic acid ethyl dissolution, as need testing solution;

2. the preparation of reference substance solution: get the paeonol reference substance, add acetone and make the solution that every 1ml contains 2mg, in contrast product solution;

3. thin layer condition: draw above-mentioned test sample and negative sample solution each 2～4 μ l, reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: ethyl acetate=3: 1 is developing solvent, launch, take out, dry, spray is with the tart 5% ferric chloride alcoholic solution of hydrochloric acid, inspect in the test sample chromatograph with the corresponding position of reference substance chromatograph on whether show the speckle of same color, determine whether contain the Cortex Moutan composition in the test agent;

4. the method for quality control of a kind of pill for soothing liver and regulating qi according to claim 1 is characterized in that: described thin layer chromatography differentiates that the method for Rhizoma Corydalis in the prescription is:

1. the preparation of need testing solution: get the pill for soothing liver and regulating qi sample, porphyrize adds diethyl ether, and supersound process filters, and gets filtering residue, volatilizes solvent, adds methanol, and supersound process filters, and filtrate evaporate to dryness, residue add methanol makes dissolving, as need testing solution;

2. the preparation of control medicinal material solution: get Rhizoma Corydalis control medicinal material 1g, add methanol 10ml, make control medicinal material solution with this step method 1.;

3. thin layer condition and result: draw each 2～6 μ l of above-mentioned three kinds of solution, put on same silica gel g thin-layer plate respectively, with n-butyl alcohol: glacial acetic acid: water=7: 1: 2 is developing solvent, launch, take out, dry, put inspect under the ultra-violet lamp 365nm in the test sample chromatograph with the corresponding position of control medicinal material chromatograph on whether show the fluorescence speckle of same color, determine whether contain the Rhizoma Corydalis composition in the test agent.

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